CN102507768B - Method for determining adsorption strength of volatile organic compound on carbon nanotube particles - Google Patents
Method for determining adsorption strength of volatile organic compound on carbon nanotube particles Download PDFInfo
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Abstract
A method for determining adsorption strength of a volatile organic compound on carbon nanotubes particles (CNTs) comprises the following steps: filling a stainless steel column with CNTs to prepare a chromatographic column; determining retention time of the volatile organic compound to obtain the retention volume of the volatile organic compound; calculating KH (henry constant) of the volatile organic pollutant on CNTs at a specific temperature; and calculating KH of the volatile organic compound on CNTs at different temperatures according to the adherence relationship between the retention volume and temperature. The method provided by the invention can rapidly determine KH of the volatile organic compound at different temperatures, with the advantages of simple process and no needs for reagents and frequent replacement of chromatographic columns, thereby reducing materials and pollution. The method can also predict KH of compound that is difficult to be determined at low temperature according to the high-temperature KH data by extrapolation method, so that the method has important meaning for adsorption distribution of novel pollutants between CNTs and gaseous phase as well as the engineering application of CNTs as adsorbent.
Description
Technical field
The present invention relates to a kind of method of measuring the adsorption strength of volatile organic compounds on nano particle under environment temperature based on chromatographic theory, belong to the environmental pollution control technique field.
Background technology
Carbon nano-tube has good mechanics, electricity, calorifics and optical characteristics, has obtained widespread use in fields such as compound substance, catalyst support, optical device, quantum computer and biomedicines.Along with the sharp increase of carbon nano-tube use amount, it will inevitably be discharged in surrounding medium, and with environment in the interaction of pollutant generation Adsorption Phase, change pollutant and the environment of himself returns and toxicological effect.Carbon nano-tube is mainly used in to pollute at environmental area and controls and sample analysis as a kind of novel adsorbent.For example use as adsorbent and catalytic carrier in Air Pollution Control, use as the packing material of Solid-Phase Extraction (SPE) post and as the packing material of gas chromatographic column in the environmental sample pretreatment process.Therefore, the absorption property of Fast Measurement variety classes volatile organic compounds on carbon nanotube particulate, can return evaluation for the environment of carbon nano-tube and volatile organic compounds basic data is provided, use also significant to carbon nano-tube as the engineering of adsorbent simultaneously.
Henry's constant (K
H) be an important parameter (J.Phys.Chem.B.2001,105:1823～1828) of describing absorption property, can be used for characterizing the adsorption strength of adsorbate on solid material.Document " Langmuir.2010,26:15625～15633. " has been measured organic compound in the fixing retention time of phase (Zeolitic Imidazolate Framework) based on chromatographic theory, and then calculates K under relevant temperature by retention volume
H, wherein chromatogram is to obtain under the condition of infinite dilution between keeping, and meets Henry's law.Document " J.Chem.Eng.Data.2010; 55:2840～2847. ", adopt volumetric method (volumetric method), by the adsorption isothermal of match methane Langmuir or Toth equation on two kinds of absorbent charcoal materials, calculate K under unlimited low pressure thereby obtain the absorption parameters such as isosteric heat of adsorption, the equilibrium constant and saturated extent of adsorption
HK under the unlimited low pressure that volumetric method is suitable for being difficult to directly measure
HBut at first the method wants the match adsorption isothermal, and needs specific instrument and equipment, wastes time and energy.Measure retention volume based on chromatographic theory and obtain K
HMethod simple, document " J Colloid.Interf.Sci.2007,305:7-16. " uses the method to measure five kinds of alkane, benzene, chloroform, triclene and zellon K on the carbon nano-particle thing
H, the classes of compounds that relates to is less, and does not set up K
HTemperature dependency relation, be difficult to obtain the K of dissimilar organic compound on his nanoparticles at other temperature
H, therefore need the lower organic compound K on the carbon nano-particle thing of a kind of quick acquisition different temperatures of development (particularly low temperature)
HMethod.
Carbon nanotube particulate of a great variety, the volatile organic compounds kind is also thousands of, and these are carried out the match of adsorption isothermal one by one, length consuming time, cost is high.Therefore, need development a kind of fast, effective method is measured the K of different types of organic compound on carbon nanotube particulate
HIn addition, K
HHave stronger temperature dependency, need to set up K
HWith the relational expression of temperature, this is significant to the prediction of the adsorption strength of the volatile organic compounds in atmosphere for the carbon nanotube particulate under environment temperature.
Summary of the invention
The present invention develops the method for the adsorption strength of volatile organic compounds on nano particle under a kind of Fast Measurement environment temperature.The method has fast, accurately, few, the free of contamination advantage of reagent dosage, the environment of estimating emerging pollutant is returned to become to having important references and be worth simultaneously and use also significant for carbon nano-tube as the engineering of adsorbent.
Technical scheme of the present invention is as follows:
The first step: preparation carbon nanotube particulate packed column: the loading of carbon nano-tube is controlled at the 100mg left and right, and excessive carbon nano-tube can cause the adsorption-desorption time oversize, affects the post effect.Concrete preparation method is as follows:
(1) dress post: at first stainless-steel tube is carried out leak test and cleaning, the method filling of then adopting vacuum pump to bleed; First with a termination vacuum pump of post, can use glass wool, gauze, glass filter ball etc. as filtering material during the dress post; From the other end of post, carbon nano-tube is added in post from funnel, can be chosen the multi-walled carbon nano-tubes of purity 95%, external diameter 3～10nm, length 5～20nm.Filling process can be connected with funnel with crossover sub, can rap each position of post in filling process, and filler is filled evenly in post as far as possible.The import of populated rear mark pillar, and sealed membrane or other encapsulants seal two-port, prevents from polluting filler in post;
(2) aging: as under the carrier gas protection, to adopt the aging packed column of temperature programme;
(3) thermal stability check: adopt thermogravimetric analysis (TGA) test packed column in room temperature to 400 ℃ thermal stability; heating rate is 10 ℃/min; take inert gas as protection gas; check the stability of carbon nano-tube filled post, carry out in order to guarantee that being determined at of follow-up chromatographic retention stablized in filler systems.Result shows that the weightlessness of carbon nanotube particulate after pyroprocessing repeatedly is almost constant, good thermal stability.
Second step: adopt in the packed column access gas chromatography of above-mentioned preparation, use the detector recording signal, according to following formula (1), calculate retention volume V by measuring the retention time of compound under 200 ℃～300 ℃
n
V
n＝(t
R-t
M)·F·j/m·T/T
a，(1)
T wherein
R, t
MIt is respectively retention time and the dead time of compound; F is the flow velocity of carrier gas, measures by soap film flowmeter; J is improvement factor, calculates by formula (2)
p
iAnd p
0Respectively the pressure of chromatographic column import and outlet; M is the weight of filler; T, T
aBe respectively furnace temperature and room temperature, and then obtain K
H
K
H＝V
n/RT，(3)
R is ideal gas constant, gets 8.314Jmol
-1K
-1
Some volatile compound chromatographic retention at low temperatures is long, is not suitable for direct mensuration; Some volatile compounds are separately arranged because its boiling point is relatively high, do not go out at low temperatures the peak, can't obtain their retention time.Above-mentioned formula is applicable to the larger compound of volatility, in order to obtain the K of compound at other temperature
H, need to set up K
HBe used for prediction with the relational expression of temperature.At first adopt the Vn of compound on carbon nano-tube filled post of said determination, set up the relational expression (4) of lnVn and 1/T
lnV
n＝k/T+C，(4)
Be extrapolated to the lnVn of volatile organic compounds on carbon nano-tube filled post under 20 ℃～200 ℃ conditions based on formula (4) again.By lnVn at other temperature of extrapolation, can try to achieve K under specified temp by formula (3)
HMeasured value and predicted value are compared, and checking is based on the K of formula (4)
HForecasting accuracy.The volatility of methylene chloride and methenyl choloride is larger, measures both at the Vn of carbon nano-tube post at 50 ℃～100 ℃ temperature, and the predicted value of lnVn measured value and extrapolation is compared as following table 1, and result shows to extrapolate to have higher accuracy.
The lnV of table 1 methylene chloride and methenyl choloride
nThe comparison of measured value and 50 ℃～100 ℃ of lower predicted values
Part of compounds is difficult to be obtained or can't obtain its Vn at 50 ℃～100 ℃ temperature, therefore by the checking of the Vn at 200 ℃～300 ℃ temperature.Volatile organic compounds of the present invention comprises alkanes, alkyl chloride hydro carbons, alcohols, benzene and substituted benzene, ester type compound, different according to the volatility of compound, sample size is controlled between 0.1～1 μ L, guarantee to carry out under the condition of infinite dilution, adsorption process can reach rapidly balance; Adopt constant voltage mode, packed column injection port pressure is 0.308MPa.
The beneficial effect that the present invention carries is as follows:
1. it is high that the carbon nano-tube filled post for preparing has thermal stability, and the volatile organic compounds that can be used in analysis comprises alkanes, alkyl halide hydro carbons, alcohols, benzene, substituted benzene and ester class.
2. use vapor-phase chromatography simple to operate, take pure reagent as probe molecule, need not to add reagent, the carbon nano-tube filled post of preparation can Reusability, reduces and pollutes.
The method can the quick obtaining different temperatures under the K of volatile organic compounds on carbon nanotube particulate
H, can be used for the adsorption strength of volatile organic compounds on carbon nanotube particulate that acquisition fast has similar structures.
Description of drawings
Fig. 1 is the thermogravimetric analysis image of carbon nano-tube.
Fig. 2 is the gas chromatogram of different sample size methyl alcohol, benzene, ethyl propionate adsorption process on carbon nano-tube.
Fig. 3 is that volatile organic compounds is adsorbed strong lnK on carbon nano-tube
HVariation with temperature 1/T.
Embodiment
Embodiment 1
The leak test of packed column and cleaning: choosing length is 0.5m, diameter
Stainless steel column, column jecket outlet blocked submerge, import passes into the carrier gas of a little higher than routine operating pressure of pressure, packed column should not have bubble to emerge, otherwise this packed column gas leakage is described, can not use; Pillar soaks to take out with 10% hydrochloric acid and 10% heat alkali liquid respectively to be washed, then rinses to neutral with tap water, uses at last distilled water, acetone rinsing, dry for standby.
Dress post: the method filling of adopting vacuum pump to bleed, dress is first blocked with glass wool and gauze one of post during post gently, connect glass filter ball and vacuum pump, the other end of post connects with plastic funnel and crossover sub, be 95% with purity, external diameter 3～10nm, length is that the multi-walled carbon nano-tubes of 5～20nm is added in post from funnel.To constantly rap each position of post in filling process, filler is filled evenly in post as far as possible.Populatedly seal two-port with sealed membrane afterwards, prevent from polluting filler in post, and the import of the good pillar of mark.
Aging: as under nitrogen protection, to adopt the aging packed column of temperature programme, the phase one: 60 ℃～180 ℃, heating rate: 4 ℃/min, the intensification terminal point keeps 60min; Subordinate phase: 180 ℃～350 ℃, heating rate: 3 ℃/min, the intensification terminal point keeps 300min; Phase III: 350 ℃～60 ℃, heating rate: 5 ℃/min, the intensification terminal point keeps 10min.
Thermal stability check: adopt the thermal stability of thermogravimetric analysis test packed column in room temperature～400 ℃, heating rate is 10 ℃/min, and take nitrogen as protection gas, result shows that in packed column, filler is through still keeping stable after pyroprocessing repeatedly.
Embodiment 2
200 ℃ of 200 ℃ of injector temperatures, the furnace temperature of setting gas chromatography, the temperature of FID are 300 ℃, after system stability, use the tip microsyringe to get 40 μ L gases methane, inject fast injection port, measure the dead time t of pillar
M, get 0.1 μ L liquid methylene chloride with the tip microsyringe, inject fast injection port, measure the retention time t of methylene chloride on multi-walled carbon nano-tubes
R, according to the V of 200 ℃ of lower methylene chloride of formula (1) calculating
n, and then obtain methylene chloride at this temperature, the K on multi-walled carbon nano-tubes
H(formula 3).
Set furnace temperature and be 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃ respectively, other conditions are constant, measure the K of methylene chloride on multi-walled carbon nano-tubes under different temperatures
H, with the lnV of six temperature spots obtaining
nWith the 1/T linear fit, obtain slope k (3327.85 ± 225.89) and intercept C (3.76 ± 0.50), extrapolate the lnV of 50 ℃ of lower methylene chloride
nBe 6.53ml.
Setting furnace temperature is 50 ℃, and other conditions are constant, measure 50 ℃ of lower methylene chloride lnV on multi-walled carbon nano-tubes
nBe 6.87 ± 0.17ml, the comparison prediction value is in the error range of experiment value, and the result that shows extrapolation is reliable.
Again according to the lnV of methylene chloride under 50 ℃ that predicts
nCalculate the K at this temperature
HBe 255110.77mmol/kg/kPa.
Embodiment 3
200 ℃ of 200 ℃ of injector temperatures, the furnace temperature of setting gas chromatography, the temperature of FID are 300 ℃, after system stability, use the tip microsyringe to get 40 μ L gases methane, inject fast injection port, measure the dead time t of pillar
M, get 0.6 μ L liquid methenyl choloride with the tip microsyringe, inject fast injection port, measure the retention time t of methenyl choloride on multi-walled carbon nano-tubes
R, according to the V of 200 ℃ of lower methenyl cholorides of formula (1) calculating
n, and then obtain methenyl choloride at this temperature, the K on multi-walled carbon nano-tubes
H(formula 3).
Set furnace temperature and be 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃ respectively, other conditions are constant, measure the K of methenyl choloride on multi-walled carbon nano-tubes under different temperatures
H, with the lnV of six temperature spots obtaining
nWith the 1/T linear fit, obtain slope k (3538.22 ± 112.08) and intercept C (3.10 ± 0.24), extrapolate the lnV of 80 ℃ of lower methenyl cholorides
nBe 6.92ml.
Setting furnace temperature is 80 ℃, and other conditions are constant, measure 80 ℃ of lower methenyl choloride lnV on multi-walled carbon nano-tubes
nBe 7.10 ± 0.04, the comparison prediction value is in the error range of experiment value, and the result that shows extrapolation is reliable.
Methenyl choloride according to prediction calculates K at this temperature at the lnVn under 80 ℃ again
HBe 344785.18mmol/kg/kPa.
Embodiment 4
200 ℃ of 200 ℃ of injector temperatures, the furnace temperature of setting gas chromatography, the temperature of FID are 300 ℃, after system stability, use the tip microsyringe to get 40 μ L gases methane, inject fast injection port, measure the dead time t of pillar
M, get 0.1 μ L liquid n-pentane with the tip microsyringe, inject fast injection port, measure the retention time t of n-pentane on multi-walled carbon nano-tubes
R, according to the V of 200 ℃ of lower n-pentanes of formula (1) calculating
n, and then obtain n-pentane at this temperature, the K on multi-walled carbon nano-tubes
H(formula 3).
Set furnace temperature and be 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃ respectively, other conditions are constant, measure the K of n-pentane on multi-walled carbon nano-tubes under different temperatures
H, with the lnV of six temperature spots obtaining
nWith the 1/T linear fit, obtain slope k (4586.96 ± 54.91) and intercept C (4.57 ± 0.11), extrapolate the lnV of 200 ℃ of lower n-pentanes
nBe 3.30ml, with the lnV of 200 ℃ of lower n-pentanes
nMeasured value 3.31ml compares, and predicted value shows that the extrapolation result is reliable in the error range of experiment value.
Embodiment 5
200 ℃ of 200 ℃ of injector temperatures, the furnace temperature of setting gas chromatography, the temperature of FID are 300 ℃, after system stability, use the tip microsyringe to get 40 μ L gases methane, inject fast injection port, measure the dead time t of pillar
M, get 0.1 μ L liquid methanol with the tip microsyringe, inject fast injection port, measure the retention time t of methyl alcohol on multi-walled carbon nano-tubes
R, according to the V of 200 ℃ of lower methyl alcohol of formula (1) calculating
n, and then obtain methyl alcohol at this temperature, the K on multi-walled carbon nano-tubes
H(formula 3).
Set furnace temperature and be 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃ respectively, other conditions are constant, measure the K of methyl alcohol on multi-walled carbon nano-tubes under different temperatures
H, with the lnV of six temperature spots obtaining
nWith the 1/T linear fit, obtain slope k (4363.73 ± 307.17) and intercept C (5.17 ± 0.60), extrapolate the lnV of 200 ℃ of lower methyl alcohol
nBe 2.24ml, with the lnV of 200 ℃ of lower methyl alcohol
nMeasured value 2.18ml compares, and predicted value shows that the extrapolation result is reliable in the error range of experiment value.
Embodiment 6
200 ℃ of 200 ℃ of injector temperatures, the furnace temperature of setting gas chromatography, the temperature of FID are 300 ℃, after system stability, use the tip microsyringe to get 40 μ L gases methane, inject fast injection port, measure the dead time t of pillar
M, get 0.1 μ L liquid benzene with the tip microsyringe, inject fast injection port, measure the retention time t of benzene on multi-walled carbon nano-tubes
R, according to the V of 200 ℃ of lower benzene of formula (1) calculating
n, and then obtain benzene at this temperature, the K on multi-walled carbon nano-tubes
H(formula 3).
Set furnace temperature and be 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃ respectively, other conditions are constant, measure the K of benzene on multi-walled carbon nano-tubes under different temperatures
H, with the lnV of six temperature spots obtaining
nWith the 1/T linear fit, obtain slope k (4731.90 ± 175.12) and intercept C (3.83 ± 0.32), extrapolate the lnV of 200 ℃ of lower benzene
nBe 4.35ml, with the lnV of 200 ℃ of lower benzene
nMeasured value 4.55ml compares, and predicted value shows that the extrapolation result is reliable in the error range of experiment value.
Embodiment 7
200 ℃ of 200 ℃ of injector temperatures, the furnace temperature of setting gas chromatography, the temperature of FID are 300 ℃, after system stability, use the tip microsyringe to get 40 μ L gases methane, inject fast injection port, measure the dead time t of pillar
M, get 0.6 μ L liquid ethyl propionate with the tip microsyringe, inject fast injection port, measure the retention time t of ethyl propionate on multi-walled carbon nano-tubes
R, according to the V of 200 ℃ of lower ethyl propionates of formula (1) calculating
n, and then obtain ethyl propionate at this temperature, the K on multi-walled carbon nano-tubes
H(formula 3).
Set furnace temperature and be 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃ respectively, other conditions are constant, measure the K of ethyl propionate on multi-walled carbon nano-tubes under different temperatures
H, with the lnV of six temperature spots obtaining
nWith the 1/T linear fit, obtain slope k (5048.63 ± 77.11) and intercept C (5.19 ± 0.15), extrapolate the lnV of 200 ℃ of lower ethyl propionates
nBe 3.66ml, with the lnV of 200 ℃ of lower ethyl propionates
nMeasured value 3.65ml compares, and predicted value shows that the extrapolation result is reliable in the error range of experiment value.
Claims (2)
1. method of measuring volatile organic compounds adsorption strength on carbon nanotube particulate is characterized in that comprising the following steps:
The first step: prepare the carbon nanotube particulate packed column: the method filling of adopting vacuum pump to bleed, the loading of carbon nano-tube is controlled at 100mg; Dress during post first with a termination vacuum pump of post; From the other end of post, carbon nano-tube is added in post from funnel, filler is filled in post evenly; The populated rear sealing both ends mouth of using; Then under the carrier gas protection, adopt the aging packed column of temperature programme; Adopt at last thermogravimetric analysis take inert gas as protection gas, the stability of check carbon nano-tube post after pyroprocessing;
Adopt the aging packed column of temperature programme, the phase one: 60 ℃ ~ 180 ℃, heating rate: 4 ℃/min, the intensification terminal point keeps 60min; Subordinate phase: 180 ℃ ~ 350 ℃, heating rate: 3 ℃/min, the intensification terminal point keeps 300min; Phase III: 350 ℃ ~ 60 ℃, heating rate: 5 ℃/min, the intensification terminal point keeps 10min;
Second step: adopt in the packed column access gas chromatography of above-mentioned preparation, record detector signal under constant voltage mode;
Mensuration under 200 ℃ ~ 300 ℃ of high temperature: calculate retention volume by the chromatographic retention of measuring compound
V n, and then obtain the Henry's constant of this compound on carbon nanotube particulate
K H
Wherein R is ideal gas constant,
TIt is furnace temperature;
Reckoning at other temperature: the compound that at first adopts said determination is on carbon nano-tube filled post
VN sets up ln
VN and 1/
TFormula (4)
Wherein,
kBe slope, C is intercept;
Arrive the ln of volatile organic compounds on carbon nano-tube filled post under ℃ condition of room temperature ~ 200 based on above-mentioned formula extrapolation again
Vn； By ln at other temperature of extrapolation
V n, based on
K HComputing formula try to achieve under specified temp
K H
2. method according to claim 1, is characterized in that, described volatile organic compounds comprises alkanes, alkyl chloride hydro carbons, alcohols, benzene and substituted benzene, ester type compound.
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| CN103760285B (en) * | 2014-01-09 | 2016-01-20 | 中国人民解放军海军医学研究所 | A kind of Freon chromatographic column and preparation method thereof |
| CN111189869B (en) * | 2018-11-15 | 2022-04-08 | 中国科学院大连化学物理研究所 | Method for determining SVOC release key parameters in building decoration material |
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